Method for preparing highly concentrated titanium sulphate solutions



Patented Mar- 15, 1932' UNETED Y STATES FRIEDRICH RASPE, or LEVEEKUSEN, NEAR oo noeiwnimvn PA L WEISE, onwinsnoitr- ON-THE-RHINE, GERMANY, ASSIGNORS "r r. G. rA BEnIN sr3rEAKrimveEsE SCI-IAFT, or FRANKFORT-ON-TI-IE-MAIN, GER-MANY, A GORPORATIONDF ennm iwj ME'rnon FOR, PREPARING HIGHLY GONCE-NTBA'TED 'TITAN 'suLrHA EsoLUErroNs- No Drawing. Application filed March 28, 1929, Serial No. 350,800, and in Germany April 4, 192 8.

This invention relates to new concentrated titanyland titanium sulphate solutions and to a process of preparing same.

n the manufacture of concentrated titanyl-or titanium-sulphate solutions with a little excess of free acid, that means titanylor titanium-sulphate solutions containing, calculated on one molecule TiOg, more than one molecule of sulphuric acid" or two molecules respectively, there is a diflicultyinasmuch as the meta-titanic acid in which form the titanium dioxide generally is obtained, is not soluble but in a large excess of concentrated sulphuric acid, while the ortho-titanio acid is soluble in dilutedacids without difli-' culties, but, when technically prepared, it

always contains great quantities of water. It is possible to dehydrate ortho-titamc acid in vacuo, but this reaction must occur very slowly lest a conversion of the ortho titanic acid into the meta-titanic acid takes place.

CJI

Therefore, this process has not been applied on a technical scale. v

Now a process has been found rendering possible the manufacture of concentrated solutions of titanylor titanium sulphate which are free from iron and contain a small excess of free sulphuric acid. First a concentrated solution of meta-titanic acid or titanium dioxide in concentrated sulphuric acid is prepared in the usual manner by dissolving the titanium dioxide or the meta-titanic acid at an elevated temperature, say between about I 150 and 200 C. Into this solutionis introduced at a temperature not over C. orthotitanic acid in small portions while stirring, until the solution has the desired content of titanium oxide. During the dissolving process it can be determined by titration'with caustic alkalies whether the solution still contains free sulphuric'acid, 'that is to say,

whether more than two molecules of sulphuric acid for each molecule of titanium di oxide are present. 0 r r Instead of preparing, in the concentrated solution or" meta-titanic acid in sulphuric acid, the saturation with meta-tie tanic acid can be eifected'in the second stage, by dissolving first a certain quantity of meta titanic acid at. a temperature between centrated in vacuo at about 0.; a syrup first stage, a

methods of carrying out our. process are.

equivalents. A strongly diluted solution containing't'itanium sulphate ,or titanyl sulphate results which can be evaporated. in

vacuo, when heated, say to about 70t0. 0., V. i and no titanium-dioxide fallsout. fInthisG mannerhighly'concentratedtitanylor ti-. tan1um=sulphate solutions, containing u i. t0

more are obtainable, said solutions being.

soluble in, water and being directly tap-' I ing materials.

plicable, especially as tanning and mordant- The, following examples illustrate our in? vention, without limiting it thereto :7

Example 1. 100 kgs.--of v meta-titanic acid. are dissolved in 15 0,200'kgsofftOncentrated; sulphuric acidat a temperature between .1509: and 200. C. ,-'andinto thislsolutiolnat a-tem:-

titanic aoid is introduced, until the solution is:

'saturatechfthen ortho-tita-nic :acid' is introduced while stirring untilthe desired basicity, is reached. The strongly diluted solution is evaporatedat 70-0090. eventually while stira ring. A'syrup easily soluble in water, re,-;

mains Q aining more thanl500 gra of Ti'Oginaliter. r 7. V

500 grams of-titaniumdioxide in one liter'or Emample 2.'l00 kgs: of titanium dioxide 7 are dissolved in 250 'kgs. ofconcentrated sulphuric acidat about C2; into'this solu- 7 tion there are introduced after cooling '54 kgs.

of ortho-titanic acid, (30%) at 50 G..wh1le stirring juntil' the titanium i dioxide is dis-' solved. The solution 'thuslobtained is coneasilysoluble in water is obtained, containing about 95% of titanyl-sulphate and about 5% of titanium sulphate, calculated on-theamount of the titanium present.

By the term,titanium sulphate formula Ti( S0 and the basic titanium sul phateof the formulaTiOSOh: I

in the "95:, claims, we mean the titaniumsulphate of thef centrated titanium sulphate solutions, the step which comprises dissolving ortho-titanic acid in a saturated solution of meta-titanic acid in concentrated sulphuric acid at a temperature of not over 60 C.

2. In the process of preparing hi 'hly concentrated titanium sulphate solutions, the step which comprises dissolving ortho-titanic acid in an amount that for two molecules of sulphuric acid at least about one molecule of titanium dioxide is present, in a saturated solution of meta-titanic acid in concentrated sulpluric acid, at a temperature of not over 60 1 3. In the process of preparing highly concentrated titanium sulphate solutions, the step which comprises dissolving ortho-titanic acid in an amount that for two molecules of sulphuric'acid about one molecule to about two molecules of titanium dioxide are present, in a saturated solution of meta-titantic acid in concentrated sulphuric acid, at atemperature of not over 60 C.

4. In the process of preparing highly concentrated titanium sulphate solutions, the steps which comprise dissolving ortho-titanic acid in a saturated solution of meta-titanic acid in concentrated sulphuric acid, at a temperatureof not over 60 C. and heating the solution in a vacuum to concentrateit.

5. In the process of preparing highly concentrated titanium sulphate solutions, the steps which comprise dissolving ortho-titanic acid in an amount that for two molecules of sulphuric acid at least about one molecule of titanium dioxide is present, in a saturated solution of meta-titanic acid inconcentrated sulphuric acid, at a temperature of not over 60 C. and heating the solution in a vacuum to concentrate it. 7

6. In the process of preparing highly concentrated titanium sulphate solutions, the steps which comprise dissolving ortho-titanic acid in an amount that for two molecules of sulphuric acid about 1 molecule to about two molecules of titanium dioxide are present, in a saturated solution of meta-titanic acid in concentrated sulphuric acid, at a temperature of not over'60 C. and heating the solution in a vacuum to concentrate it.

In testimony whereof we have hereunto set our hands. 1

FRIEDRICH RASPE. [n s] PAUL WEISE. 

